Issue 24, 2022

Crystal engineering and structural diversity of 2-aminopyridinium hypodiphosphates obtained by crystallization and dehydration

Abstract

Organic–inorganic salts and ionic co-crystals of hypodiphosphoric acid (H4P2O6) with 2-aminopyridine (2ap) have been synthesized and characterized by X-ray crystallography, thermogravimetry, elemental analysis and Fourier-transform infrared spectroscopy. (2apH)4(H3P2O6)2(H2P2O6)·2H2O (1), (2apH)2(H2P2O6)·2H2O (4), (2apH)2(H2P2O6)·(H4P2O6) (6) and (2apH)2(H2P2O6)·2(2ap) (7) were obtained in crystalline form in a typical solution-crystallization process. Compounds (2apH)4(H3P2O6)2(H2P2O6)·0.4H2O (2), (2apH)4(H3P2O6)2(H2P2O6)·0.1H2O (3) and (2apH)2(H2P2O6) (5) were formed during dehydration processes of (1) and (4), respectively, which took place as destructive transformations. Further annealing of compound (5) results in its partial decomposition into the anhydrous form of compound (3). Water removal is associated with a rearrangement of the crystal architecture and with the partial deformation of hypodiphosphate anions from the typical staggered conformation towards an eclipsed one.

Graphical abstract: Crystal engineering and structural diversity of 2-aminopyridinium hypodiphosphates obtained by crystallization and dehydration

Supplementary files

Article information

Article type
Paper
Submitted
24 Feb 2022
Accepted
13 May 2022
First published
16 May 2022

CrystEngComm, 2022,24, 4417-4429

Crystal engineering and structural diversity of 2-aminopyridinium hypodiphosphates obtained by crystallization and dehydration

D. Budzikur, V. Kinzhybalo and K. Ślepokura, CrystEngComm, 2022, 24, 4417 DOI: 10.1039/D2CE00261B

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